CN106673998A - Circulating gas stripping rectification system for extracting EPA and DHA from fish oil - Google Patents

Circulating gas stripping rectification system for extracting EPA and DHA from fish oil Download PDF

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Publication number
CN106673998A
CN106673998A CN201710149953.8A CN201710149953A CN106673998A CN 106673998 A CN106673998 A CN 106673998A CN 201710149953 A CN201710149953 A CN 201710149953A CN 106673998 A CN106673998 A CN 106673998A
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tower
dha
gas
air stripping
fish oil
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CN201710149953.8A
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CN106673998B (en
Inventor
刘汝萃
刘锡潜
范书琴
张建全
张兵
程秀梅
朱艳
魏钊锋
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TIANJIN AOZHAN XINGDA TECHNOLOGY Co Ltd
YUWANG PHARMACEUTICAL CO Ltd SHANDONG PROV
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TIANJIN AOZHAN XINGDA TECHNOLOGY Co Ltd
YUWANG PHARMACEUTICAL CO Ltd SHANDONG PROV
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/38—Steam distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
    • C07C51/445—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by steam distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)

Abstract

The invention relates to a circulating gas stripping rectification system for extracting EPA and DHA from fish oil. The system comprises a gas stripping rectification tower, wherein the top of the gas stripping rectification tower is connected with the top of a heat exchange tower; the bottom of the gas stripping rectification tower is connected with a gas stripping tower kettle storage tank through a gas stripping tower kettle extraction pump; the gas stripping rectification tower is also connected with a raw material preheater and a nitrogen heater; the top of the gas stripping rectification tower is also connected with a washing tower; the top of the washing tower is connected with a fan buffer tank; the fan buffer tank is connected with a vacuum buffer tank through a gas compressor; the vacuum buffer tank is also connected with a vacuum pump and the heat exchange tower separately; the heat exchange tower is also connected with the nitrogen heater; the bottom of the washing tower is connected with a washing tower kettle storage tank through a washing tower kettle extraction pump; the bottom of the washing tower is also connected with a circulating cooler through a washing tower circulating pump, and the circulating cooler is connected with the upper part of the washing tower. The circulating gas stripping rectification system of the invention does not need high vacuum, and the content of the EPA and the DHA can be improved to above 70% by one-time purification.

Description

A kind of circulating gas-lifting distillation system that EPA ＆ DHA are extracted from fish oil
Technical field
The present invention relates to fish oil purification technique field, more particularly, to a kind of system of EPA＆DHA in purification fish oil.
Background technology
Fish oil is rich in a series of 3 polyunsaturated fatty acid of ω, and its key component is EPA (eicosapentaenoic acid) ＆DHA (two Dodecahexaene acid), nutrient substance necessary to human growth development is not only, and there is prevention cardiovascular and cerebrovascular disease, strengthened Memory, prevents senile dementia, and antiinflammatory, suppression anaphylaxiss and tumour growth promote various lifes such as baby's retinal development Reason function.In recent years, polyunsaturated fatty acid is obtained for extensively in many industries such as medicine, food, fine chemistry industry and field Application, in supply falls short of demand situation, countries in the world government is to the food rich in EPA＆DHA for the fish oil derivant product such as EPA＆DHA Exploitation is increasingly paid attention to.
At present, in fish oil, the extracting method and process for refining of EPA＆DHA mainly have low-temperature solvent crystallization process, urea clathration Method, supercritical fluid extraction and molecularly distilled etc..Low-temperature solvent method is needed using substantial amounts of organic solvent, not only be there are Machine dissolvent residual, and substantial amounts of organic solvent need to be reclaimed, separation efficiency is not high and do not commonly used.Urea adduct method will be consumed greatly , there is solvent recovery, problem of environmental pollution in the organic solvent of amount, and be difficult to separate double-strand number close fatty acid.It is Chinese special Sharp file CN105713721A (application numbers：201610161177.9) method for disclosing DHA and EPA in a kind of fish oil concentrated, Belong to CO2Supercritical fluid extraction；However, supercritical fluid extraction equipment investment is big, condition of high voltage is needed, and can only be extracted Pigment, stink substance and part free fatty in taking-up fish oil, only serves the purpose of refined fish oil, it is impossible to high-purity EPA＆DHA.Chinese patent document CN103951556A (application number：201410192466.6) one kind is disclosed with bathypelagic fish oil For raw material, the distillation work of eicosapentaenoic acid (EPA), clupanodonic acid (DPA) and docosahexenoic acid (DHA) is separated Skill, belongs to molecularly distilled；Although molecularly distilled can obtain highly purified EPA＆DHA, however, it is desirable to high-vacuum apparatus, Multistage distillation, high energy consumption, cost of equipment maintenance are high, and production capacity is little, it is difficult to meet the needs of industrial actual production.
Chinese patent document CN202881231U (application number：201220629614.2) disclose a kind of for ethyl ester fish oil The continuous way subcritical reaction device of hydrolysis, including water tank, the reative cell with water inlet and outlet and there is liquid outlet Reserving liquid tank, being provided between the water inlet of the liquid outlet and reative cell of reserving liquid tank can be by the Water Sproading flowed out from liquid outlet to reaction The loop structure that room recycles, is additionally provided with the control structure that can control to react room pressure and temperature, condensation evaporation on reative cell Tank is provided with the recovery structure that will can be reclaimed from the detached ethanol of condensation evaporation tank.The reaction unit is primarily adapted for use in subcritical anti- Answer process, it is impossible to effectively realize the extraction of EPA＆DHA.
The content of the invention
For the deficiencies in the prior art, the present invention provides a kind of circulating gas-lifting rectification system that EPA＆DHA is extracted from fish oil System.
Technical scheme is as follows：
A kind of circulating gas-lifting distillation system that EPA＆DHA is extracted from fish oil, the system includes air stripping rectifying column, described The tower top of air stripping rectifying column is connected with stripper overhead storage tank by gas-gas heat exchanger, the bottom of stripper overhead storage tank by valve with Stripper overhead return tank connects, and the bottom of stripper overhead return tank is connected with air stripping rectifying column by stripping tower reflux pump；
The bottom of towe of described air stripping rectifying column is produced pump by air stripping tower reactor and is connected with air stripping tower reactor storage tank, described air stripping Rectifying column is also connected with feed preheater and nitrogen heater；
Described stripper overhead storage tank is also connected with scrubbing tower, and the tower top of described scrubbing tower is connected with blower fan surge tank, Described blower fan surge tank is connected with vacuum buffer tank by gas compressor, described vacuum buffer tank also respectively with vacuum pump Connect with gas-gas heat exchanger, gas-gas heat exchanger is also connected with nitrogen heater；
The bottom of towe of described scrubbing tower is connected with tower reactor storage tank is washed by washing tower reactor and producing pump, described scrubbing tower Bottom of towe is also connected with recirculation cooler by scrubbing tower circulating pump, and recirculation cooler is connected with the top of scrubbing tower.
, according to the invention it is preferred to, the tower diameter of described air stripping rectifying column is 380mm-500mm, tower height 13-17m, column plate Number is 3-6 levels.
, according to the invention it is preferred to, described scrubbing tower is plate column, using 3-6 layer bubble trays.
The circulating gas-lifting distillation system of the present invention can adopt noble gases circulating gas-lifting light component, and be entered by reflux type One step realizes that component high-purity is separated, and whole process has merged rectification and air stripping principle, using the difference of component volatilization degree in fish oil It is different, the process of many second part vaporizations and partial condensation is carried out, while utilizing hot inert gas air stripping light component, light component is reduced Partial pressure, promotes vaporization side development of the light component to balance, the light component content in heavy phase is further reduced.Inertia of the present invention Gas is recycled in the entire system, disposable to supplement, it is not necessary to extra to consume.
Advantages of the present invention or beneficial effect：
1st, fine vacuum is not needed using the circulating gas-lifting distillation system of the present invention, and disposable purification can be by EPA＆DHA Content is improved to more than 70%.
2nd, coordinate the backflow of variable concentrations using the circulating gas-lifting distillation system of the present invention, various ratios can be obtained EPA&DHA；By the use of noble gases as heat-carrying gas, separation efficiency is high, and material heated time is short, and operating condition is gentle, to temperature-sensitive Property material is survivable；Circulated using noble gases, solvent-free recovery problem, produce without waste water and garbage, solve waste water And fixed-end forces problem；Using noble gases as shielding gas, fish oil is prevented to be oxidized, peroxide value is almost 0.
3rd, circulating gas-lifting distillation system simple structure of the present invention, strong operability are capable of achieving the serialization of EPA＆DHA in fish oil Purification operations, with significant industrialization prospect；With good safety, have extensive in health product, the production of medicine Application prospect.
Description of the drawings
Fig. 1 is the agent structure schematic diagram of the circulating gas-lifting distillation system of the present invention.
Wherein：T101 air stripping rectifying columns；T102 scrubbing towers；E101 feed preheaters；E102 nitrogen heaters；E103 gas gas Heat exchanger；E104 recirculation coolers；V101 stripper overhead storage tanks；V102 stripper overhead return tanks；V103 air stripping tower reactor storage tanks； V104 washs tower reactor storage tank；V105 blower fan surge tanks；V106 vacuum buffer tanks；P101 air stripping tower reactor produces pump；P102 stripping towers Reflux pump；P103 washing tower reactor extraction pumps；P104 scrubbing tower circulating pumps；P105 gas compressors；P106 vacuum pumps.
Specific embodiment
Below by specific embodiment and combine accompanying drawing the present invention will be further described, but not limited to this.In embodiment Raw materials used to be convenient source, device therefor is conventional equipment, wherein, air stripping rectifying column T101 is conventional rectification tower.
Embodiment 1
As shown in figure 1, it is a kind of from fish oil extract EPA＆DHA circulating gas-lifting distillation system, the system include air stripping essence Tower T101 is evaporated, the tower top of described air stripping rectifying column T101 is connected with stripper overhead storage tank V101 by gas-gas heat exchanger E103, The bottom of stripper overhead storage tank V101 is connected with stripper overhead return tank V102 by valve, the bottom of stripper overhead return tank V102 Portion is connected with air stripping rectifying column T101 by stripping tower reflux pump P102；
The bottom of towe of described air stripping rectifying column T101 produces pump P101 and air stripping tower reactor storage tank V103 by air stripping tower reactor and connects Connect, described air stripping rectifying column T101 is also connected with feed preheater E101 and nitrogen heater E102；
Described stripper overhead storage tank V101 is also connected with scrubbing tower T102, the tower top and blower fan of described scrubbing tower T102 Surge tank V105 connects, and described blower fan surge tank V105 is connected with vacuum buffer tank V106 by gas compressor P105, institute The vacuum buffer tank V106 for stating also is connected with vacuum pump P106 and gas-gas heat exchanger E103 respectively, gas-gas heat exchanger E103 also with nitrogen Hot-air heater E102 connects；
The bottom of towe of described scrubbing tower T102 is connected with washing tower reactor storage tank V104 by washing tower reactor extraction pump P103, institute The bottom of towe of the scrubbing tower T102 for stating also is connected with recirculation cooler E104 by scrubbing tower circulating pump P104, recirculation cooler E104 It is connected with the top of scrubbing tower T102.
In the present embodiment, air stripping rectifying column T101 tower diameters are 400mm, and tower height 15m, the number of plates are 4 grades, and scrubbing tower T102 is Plate column, using 6 layers of bubble tray.
Used in embodiment circulating gas-lifting distillation system extract from fish oil EPA＆DHA technological process it is as follows：
Using vacuum pump P106 to whole system evacuation, vacuum environment is set up, close vacuum pump P106, buffered from blower fan Whole system is replaced as nitrogen system by the inflation inlet inflated with nitrogen of tank V105, and it is 3~5KPa that most system is evacuated to vacuum at last, Gas compressor P105 is opened, now nitrogen is opened nitrogen heater E102, nitrogen is preheated in whole system interior circulation, former Material fish oil enters air stripping rectifying column T101 after feed preheater E101 preheatings, hot nitrogen in the air stripping rectifying column T101 with Light phase from the discharge of air stripping rectifying column T101 tower tops in raw material, heavy phase (EPA＆DHA) is produced from air stripping rectifying column T101 tower reactors；
Carry light phase nitrogen through gas-gas heat exchanger E103 heat exchange after, it is a part of it is light phase be condensed, into stripping tower Top storage tank V101, subsequently into stripper overhead return tank V102, by stripping tower reflux pump P102 from air stripping rectifying column T101 towers Top pumps into T101 air stripping rectifying columns, further realizes the detached multistage distillation of component high-purity；Another part is not cooled down Gas phase enter scrubbing tower T102, scrubbing tower T102 be plate column, using 3-6 layer bubble trays；Scrubbing tower T102 tower bottoms leads to Scrubbing tower circulating pump P104 is crossed after recirculation cooler E102 coolings, circulation is played in scrubbing tower T102 towers, further by nitrogen Light phase trapping in gas is got off, and in the nitrogen after scrubbing tower T102 washings, light phase content is almost 0；
Nitrogen enters blower fan surge tank V105 from scrubbing tower T102 tower tops, enters vacuum through gas compressor P105 compressions Surge tank V106, then after the hot nitrogen of gas-gas heat exchanger E103 and air stripping rectifying column T101 overhead extractions carries out heat exchange, Further heat into nitrogen heater E102, squeeze into the use of air stripping rectifying column T101 interior circulations.
Application examples 1：
Air stripping rectifying column T101 tower diameter DN400mm, high 15m, 142 DEG C of tower top temperature, 178 DEG C of column bottom temperature；System is taken out very Sky is preheating to 250 DEG C through nitrogen heater E102 to 4KPa, nitrogen Jing after gas compressor P105 circulations, and nitrogen flow is 1500m3/h；
(EPA＆DHA contents 24% in raw material, wherein EPA contain 13% to raw material fish oil inlet amount 25L/h, and quality percentage contains Amount), after feed preheater E101 is preheating to 140 DEG C, feed from the middle part of air stripping rectifying column T101, air stripping rectifying column T101 towers Stream is returned by stripping tower reflux pump P102 in top, reflux temperature is 110 DEG C, and for 15L/h, (backflow is consisted of backflow flow The liquid phase collected when not flowing back under the conditions of being somebody's turn to do, EPA content are less than 2%, weight/mass percentage composition), from air stripping rectifying column T101 tower reactors Extraction EPA＆DHA mixture, up to 70%, wherein EPA contains 37% to EPA＆DHA contents, weight/mass percentage composition.
Application examples 2：
Air stripping rectifying column T101 tower diameter DN400mm, high 15m；System is evacuated to 4KPa, 142 DEG C of tower top temperature, bottom of towe temperature 178 DEG C of degree, nitrogen are preheating to 250 DEG C through nitrogen heater E102 Jing after gas compressor P105 circulations, and nitrogen flow is 1500m3/h；
Raw material fish oil inlet amount 25L/h (EPA＆DHA contents 25%, weight/mass percentage composition in raw material), through raw material preheating After device E101 is preheating to 140 DEG C, feed from the middle part of air stripping rectifying column T101, air stripping rectifying column T101 tower tops are flowed back by stripping tower Pump P102 returns stream, reflux temperature is 110 DEG C, and backflow flow is that (backflow consists of EPA content about 6%, DHA to 15L/h Content is 0, weight/mass percentage composition), EPA＆DHA mixture is produced from air stripping rectifying column T101 tower reactors, EPA＆DHA contents are reachable 73%, wherein EPA contain 48%, weight/mass percentage composition.

Claims (6)

1. it is a kind of from fish oil extract EPA＆DHA circulating gas-lifting distillation system, it is characterised in that the system includes air stripping rectification Tower, the tower top of described air stripping rectifying column are connected with stripper overhead storage tank by gas-gas heat exchanger, the bottom of stripper overhead storage tank It is connected with stripper overhead return tank by valve, the bottom of stripper overhead return tank is by stripping tower reflux pump and air stripping rectifying column Connection；
The bottom of towe of described air stripping rectifying column is produced pump by air stripping tower reactor and is connected with air stripping tower reactor storage tank, described air stripping rectification Tower is also connected with feed preheater and nitrogen heater；
Described stripper overhead storage tank is also connected with scrubbing tower, and the tower top of described scrubbing tower is connected with blower fan surge tank, described Blower fan surge tank be connected with vacuum buffer tank by gas compressor, described vacuum buffer tank is also gentle with vacuum pump respectively Gas heat exchanger connects, and gas-gas heat exchanger is also connected with nitrogen heater；
The bottom of towe of described scrubbing tower is connected with tower reactor storage tank is washed by washing tower reactor and producing pump, the bottom of towe of described scrubbing tower Also it is connected with recirculation cooler by scrubbing tower circulating pump, recirculation cooler is connected with the top of scrubbing tower.
2. it is according to claim 1 from fish oil extract EPA＆DHA circulating gas-lifting distillation system, it is characterised in that institute The tower diameter of the air stripping rectifying column stated is 380mm-500mm.
3. it is according to claim 1 from fish oil extract EPA＆DHA circulating gas-lifting distillation system, it is characterised in that institute The tower height 13-17m of the air stripping rectifying column stated.
4. it is according to claim 1 from fish oil extract EPA＆DHA circulating gas-lifting distillation system, it is characterised in that institute The number of plates of the air stripping rectifying column stated is 3-6 levels.
5. it is according to claim 1 from fish oil extract EPA＆DHA circulating gas-lifting distillation system, it is characterised in that institute The scrubbing tower stated is plate column.
6. it is according to claim 5 from fish oil extract EPA＆DHA circulating gas-lifting distillation system, it is characterised in that institute The plate column stated adopts 3-6 layer bubble trays.
CN201710149953.8A 2017-03-14 2017-03-14 A kind of circulating gas-lifting distillation system that EPA ＆ DHA are extracted from fish oil Active CN106673998B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110257446A (en) * 2019-07-08 2019-09-20 青岛和合汇途工程技术有限公司 A kind of preparation method of high-purity EPA glyceride and DHA glyceride
CN111450561A (en) * 2020-04-15 2020-07-28 陕西聚能新创煤化科技有限公司 Energy-saving carrier gas stripping system and stripping process
CN114605256A (en) * 2022-03-14 2022-06-10 山东禹王制药有限公司 Extraction method of fish oil intermediate EPA70

Citations (4)

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Publication number Priority date Publication date Assignee Title
US4874629A (en) * 1988-05-02 1989-10-17 Chang Stephen S Purification of fish oil
US20040253353A1 (en) * 2003-06-16 2004-12-16 Dick Copeland Steam-free deodorization process
CN101235341A (en) * 2008-02-27 2008-08-06 天津大学 Device for preparing sea dog oil and preparation method thereof
WO2008093378A1 (en) * 2007-01-31 2008-08-07 Adorkem Technology Spa Process of selective enzymatic enrichment of a mixture containing omega-3

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4874629A (en) * 1988-05-02 1989-10-17 Chang Stephen S Purification of fish oil
US20040253353A1 (en) * 2003-06-16 2004-12-16 Dick Copeland Steam-free deodorization process
WO2008093378A1 (en) * 2007-01-31 2008-08-07 Adorkem Technology Spa Process of selective enzymatic enrichment of a mixture containing omega-3
CN101235341A (en) * 2008-02-27 2008-08-06 天津大学 Device for preparing sea dog oil and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110257446A (en) * 2019-07-08 2019-09-20 青岛和合汇途工程技术有限公司 A kind of preparation method of high-purity EPA glyceride and DHA glyceride
CN110257446B (en) * 2019-07-08 2023-01-13 青岛和合汇途工程技术有限公司 Preparation method of high-purity EPA glyceride and DHA glyceride
CN111450561A (en) * 2020-04-15 2020-07-28 陕西聚能新创煤化科技有限公司 Energy-saving carrier gas stripping system and stripping process
CN111450561B (en) * 2020-04-15 2024-04-26 陕西聚能新创煤化科技有限公司 Energy-saving carrier gas stripping system and stripping process
CN114605256A (en) * 2022-03-14 2022-06-10 山东禹王制药有限公司 Extraction method of fish oil intermediate EPA70

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